CN101805136B - Chemical method for in situ preparing nano mesh-like sulfur-indium-zinc ternary compound optoelectronic film on ITO conductive glass - Google Patents
Chemical method for in situ preparing nano mesh-like sulfur-indium-zinc ternary compound optoelectronic film on ITO conductive glass Download PDFInfo
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- CN101805136B CN101805136B CN 201010125445 CN201010125445A CN101805136B CN 101805136 B CN101805136 B CN 101805136B CN 201010125445 CN201010125445 CN 201010125445 CN 201010125445 A CN201010125445 A CN 201010125445A CN 101805136 B CN101805136 B CN 101805136B
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Abstract
The invention relates to a chemical method for preparing a nano mesh-like sulfur-indium-zinc ternary compound optoelectronic film on ITO conductive glass in situ. The method comprises the following steps that: an ITO conductive glass substrate material with a nano indium-zinc alloy surface, monomer sulfur powder and anhydrous ethanol are put into a PTFE reactor, with the concentration of monomer sulfur powder of 0.001 to 0.015g sulfur/ml anhydrous ethanol, react for 12 to 24h at 160 to 180DEG C, are naturally cooled to room temperature after the reaction is completed; and finally, the product is sequentially cleaned by deionized water and anhydrous ethanol, naturally dried at room temperature, and the mesh-like ZnIn2S4 ternary compound optoelectronic film which comprises nano sheets is prepared on the indium-zinc alloy surface of an ITO conductive glass substrate in situ, wherein the thickness of the nano sheets is 20 to 30mm. The film prepared by the method is transparent, the nano mesh-like structure has uniform and perfect appearance, and the surface is very uniform and flat. Simultaneously, the method has the advantages of good low-temperature in situ growth repeatability, convenient operation, no further post-treatment, environmental-friendliness and convenience for industrial production.
Description
Technical field:
The invention belongs to material chemistry technical field, relate in particular to a kind of chemical process of the mesh-like sulfur-indium-zinc ternary compound optoelectronic film material that in-situ preparing is made up of nano flake in the substrate of ITO conductive glass.
Background technology:
ZnIn
2S
4(ZIS) as the II-III-VI compound semiconductor, belong to AB
2C
4The ternary sulfide of series.Because of having moderate band-gap energy, high conversion rate and lower manufacturing cost etc., it is widely used in aspects such as solar cell, photochemical catalysis, pl-diode, biomarker and photosensor.
At present, about sulphur indium zinc (ZnIn
2S
4) the existing many reports of crystalline preparation method, people [X.L.Gou, F.Y.Cheng, Y.H.Shi, L.Zhang, S.J.Peng, J.Chen, P.W.Shen.J.Am.Chem.Soc.2006,128,7222-7229.] such as the Gou Xing of Nankai University dragon are with zinc sulfate (ZnSO
4), indium chloride (InCl
3) and thioacetamide (TAA) prepared the sulphur indium zinc micro Nano material of different-shape for raw material solvent thermal under the condition that tensio-active agent exists.The Chen Zhi of University of Fuzhou newly waits people [Z.X.Chen, D.Z.Li, W.J.Zhang; C.Chen, W.J.Li, M.Sun; Y.H.He; X.Z.Fu.Inorganic Chemistry 2008,42,9766-9772.] under the prerequisite that has no tensio-active agent and template, be equipped with sulphur indium zinc micron spherical structure with the water-bath legal system.Though these two class methods can be prepared sulphur indium zinc micro-/ nano material simply and easily, the final product that they obtain all is sulphur indium zinc (ZnIn
2S
4) powdered material, if it is applied in the solar cell as photovaltaic material, also need further preparation film forming.Recently, people [M.T.Li, J.Z.Su, L.J.Guo.International Journal of HydrogenEnergy 2008,33,2891-2896.] such as Shanghai Communications University, Xi'an Li Ming great waves utilizes spray heating decomposition in the substrate of ITO conductive glass, to prepare ZnIn
2S
4Thin-film material, this method is with ZnCl
2, InCl
3(NH
2)
2CS is a precursor solution, under the condition of 400 ℃ of base reservoir temperatures, on the ITO conductive glass, deposits ZnIn
2S
4Film.Though this method preparation cost is lower, need depends on complicated conversion unit and harsh reaction conditions, and under higher base reservoir temperature, might destroy the electroconductibility of ito glass.And the ZnIn that obtains
2S
4The pattern heterogeneity of nano material, wayward, be difficult to form three-dimensional structure, therefore, seeks a kind of simple, fast, the method for gentle, cheapness and environmental protection, in the substrate of ITO conductive glass, directly prepare ZnIn with ideal three-dimensional structure
2S
4The ternary compound optoelectronic film material remains the problem that researchists need solution.
In addition, the reticulated film structure of being made up of nano flake that need particularly point out because of having bigger specific surface area, being easy to form with other materials characteristics such as inierpeneirating network structure, will have some unique electron transport ability.With inorganic semiconductor-conjugated polymers hybrid solar cell is example; Such solar cell is the inorganic semiconductor and conjugated polymers mixing formation heterojunction with nanoscale, and this structure has not only been utilized the characteristics that the inorganic nano-crystal carrier mobility is high, chemicalstability is good but also kept good snappiness and the workability of macromolecular material.Under irradiation of sunlight; The free charge carrier produces at the interface and separates through inorganic (semi-conductor) in heterojunction-organic (polymkeric substance) after the optical excitation, and the mixed effect of inorganic-organic two components and effective contact area are one of the important factors of the photoelectric properties of decision solar cell.Has special cancellated ZnIn
2S
4Optoelectronic thin film material is because its higher specific surface area and complicated three-dimensional structure; And be easy to contact good inierpeneirating network structure, so they are the desirable alternative materials as inorganic semiconductor-conjugated polymers hybrid solar cell with organic polymer material formation.
The applicant has used a kind of simple, quick, gentle, green compound method; Ito glass base material with indium zinc alloy surface; Elemental sulfur powder (S); And anhydrous ethanol solvent places the tetrafluoroethylene reaction kettle altogether, and direct reaction is 12～24 hours under 160 ℃～180 ℃ temperature, and successfully in-situ preparing has gone out the netted ZnIn that is made up of nano flake (20～30nm is thick) in the substrate of ITO conductive glass
2S
4The ternary compound optoelectronic film material, the porosity of reticulated film material is between 100～400nm.Show that through sem (SEM) and X-ray powder diffraction appearance (XRD) characterization method when temperature of reaction during at 140 ℃, indium zinc alloy surface and sulphur powder do not react basically.When temperature of reaction is 160 ℃, indium zinc alloy surface and sulphur powder react but not exclusively.Have only and when the solvent thermal reaction temperature surpasses 160 ℃, just can generate perfect nano mesh-like sulfur-indium-zinc ternary compound optoelectronic thin-film material; The top condition that generates the mesh-like sulfur-indium-zinc ternary compound optoelectronic film material is 180 ℃ of reactions 24 hours, reduces temperature of reaction or shorten the reaction times all to can not get perfect mesh-like sulfur-indium-zinc ternary compound optoelectronic film material.
Summary of the invention:
The present invention is directed to the ZnIn for preparing at present
2S
4Mostly nanocrystalline material is powdery product, can't directly be used for solar cell device as photovaltaic material; Existing preparation ZnIn
2S
4Have in the method for thin-film material that base reservoir temperature is higher, shortcoming such as complex process, severe reaction conditions and pattern are undesirable.Provide a kind of, need not add any tensio-active agent, needn't pass through loaded down with trivial details post-processing operation such as removal of impurities, under lower temperature, can make the ZnIn of highly purified mesh nanometer structure without any need for template
2S
4The method of ternary compound optoelectronic film material.This method goes on foot directly growth in situ ZnIn in the ito glass substrate of chemical reaction through one
2S
4The ternary compound optoelectronic film material has the wide industrial application prospect,
The technical scheme that the present invention taked is:
A kind of sulphur indium zinc (ZnIn
2S
4) the ternary compound optoelectronic film material, it is characterized in that: this material is the netted ZnIn that is made up of nano flake of in-situ preparing in the ITO conductive glass substrate with nanometer indium zinc alloy surface
2S
4The ternary compound optoelectronic film material, wherein nano flake thickness is 20～30nm.
Sulfur-indium-zinc ternary compound optoelectronic film preparation methods of the present invention; It is characterized in that: this method places ITO conductive glass base material, elemental sulfur powder and anhydrous ethanol solvent with nanometer indium zinc alloy surface the polytetrafluoroethylliner liner of reaction kettle altogether; The concentration of elemental sulfur powder is 0.001～0.0015 gram sulphur/milliliter anhydrous ethanol solvent; Under 160 ℃～180 ℃ temperature, reacted 12～24 hours; Reaction naturally cools to room temperature after finishing, and final product cleans with deionized water and absolute ethyl alcohol successively; Naturally dry the netted ZnIn that forms by nano flake that promptly obtains in the indium zinc alloy surface in-situ preparing of ITO conductive glass substrate under the room temperature
2S
4The ternary compound optoelectronic film material, wherein nano flake thickness is 20～30nm.
Described sulfur-indium-zinc ternary compound optoelectronic film preparation methods, preferable reaction temperature are 180 ℃, and the reaction times is 18～24 hours.More excellent temperature of reaction is 180 ℃, and the reaction times is 24 hours.
Described ITO conductive glass base material with nanometer indium zinc alloy surface is meant the material that has plated one deck nanometer indium zinc alloy through ion sputtering at the ITO conductive glass surface.
Advantage of the present invention:
1, low-temperature original position growth good reproducibility, film is transparent, mesh nanometer structure and morphology homogeneous, perfection, the surface is very evenly smooth, has solved the uneven problem of other spin coating method crystal films.
2, easy and simple to handle, do not need further aftertreatment, the product impure phenomenon that can also avoid other wet chemistry prepared in reaction to be caused.And need not to use the bigger solvent of toxicity such as triphenylphosphine, Hydrazine Hydrate 80, quadrol and toluene etc., belong to environmentally friendly reaction.Be convenient to suitability for industrialized production and technology popularization.
3, low temperature in-situ growth mesh nanometer ZnIn in the substrate of ITO conductive glass
2S
4The ternary compound optoelectronic film material, thus overcome method complicated process of preparation and the higher shortcomings of base reservoir temperature such as the physical vapor precipitator method, spraying cracking process.
4, do not need further spin-coating film process, be convenient to the assembling solar battery device.
Method of the present invention has directive significance to the preparation of other polynary sulfide thin film materials.
Description of drawings
Be coated with a layer thickness on Fig. 1, the ITO conductive glass and be about the AFM photo of the indium zinc alloy film of 20nm
The electron photomicrograph of the sulphur indium zinc nanocrystalline film material of Fig. 2, embodiment 1 preparation
The electron photomicrograph of the sulphur indium zinc nanocrystalline film material of Fig. 3, embodiment 2 preparations
The electron photomicrograph of the sulphur indium zinc nanocrystalline film material of Fig. 4, embodiment 3 preparations
The electron photomicrograph of the sulphur indium zinc nanocrystalline film material of Fig. 5, embodiment 4 preparations
The electron photomicrograph of the sulphur indium zinc nanocrystalline film material of Fig. 6, embodiment 5 preparations
The X ray diffracting spectrum of the sulphur indium zinc nanocrystalline film material of Fig. 7, embodiment 4 preparations
The sulphur indium zinc nanocrystalline film material of Fig. 8, embodiment 4 preparations ultraviolet-spectrogram diffuses
The pictorial diagram (B) of Fig. 9, the transparent sulphur indium of glassy yellow zinc nanocrystalline film material pictorial diagram (A) that embodiment 4 prepares in the substrate of ITO conductive glass and initial indium zinc alloy thin-film material
Embodiment:
The present invention prepares the implementation method of sulfur-indium-zinc ternary compound optoelectronic film material; The ITO conductive glass base material that at first will have nanometer indium zinc alloy surface; The elemental sulfur powder; And anhydrous ethanol solvent blend in the polytetrafluoroethylliner liner of reaction kettle, sealing is placed in the constant temperature air dry oven of temperature programming function, and direct reaction is 12～24 hours under 160 ℃～180 ℃ temperature; After reaction finished, the question response still after in the constant temperature air dry oven, being cooled to room temperature took out reaction kettle; At last product is taken out successively and clean, dry naturally under the room temperature with deionized water and absolute ethyl alcohol.
Embodiment 1
(1) preparation work: will be coated with the ITO conductive glass that a layer thickness is about the indium zinc alloy film of 20nm and in ultrasonic cleaner, clean 5 minutes with deionized water and absolute ethyl alcohol successively, and take out to be placed on the filter paper then and dry naturally; The polytetrafluoroethylliner liner of reaction kettle is used tap water, distilled water wash successively, and dry back is for use;
(2) reactions step: put into polytetrafluoroethylliner liner to the ITO conductive glass substrate of handling with nanometer indium zinc alloy surface; Add the sulphur powder; The height that adds anhydrous ethanol solvent to container 75% then; Sulphur powder concentration is 0.001 grams per milliliter, and polytetrafluoroethylliner liner is put into stainless steel outer sleeve and placed the constant temperature air dry oven with temperature programming function, is warmed up to 180 ℃ of reactions 24 hours;
(3) aftertreatment: after reaction finishes, close the constant temperature air dry oven and naturally cool to room temperature, use deionized water and absolute ethyl alcohol wash products successively after, sample placed under the room temperature dries naturally.The sulphur indium zinc film sample that obtains is carefully changed in the sample bottle, in lucifuge, exsiccant environment, preserve.Product colour is a glassy yellow, and the microtexture under electron microscope is latticed nanocrystalline.Electron photomicrograph is seen Fig. 2.
Embodiment 2
(1) preparation work: will be coated with the ITO conductive glass that a layer thickness is about the indium zinc alloy film of 80nm and in ultrasonic cleaner, clean 5 minutes with deionized water and absolute ethyl alcohol successively, and take out to be placed on the filter paper then and dry naturally; The polytetrafluoroethylliner liner of reaction kettle is used tap water, distilled water wash successively, and dry back is for use;
(2) reactions step: put into polytetrafluoroethylliner liner to the ITO conductive glass substrate of handling with nanometer indium zinc alloy surface; Add the sulphur powder; The height that adds anhydrous ethanol solvent to container 75% then; Sulphur powder concentration is 0.0015 grams per milliliter, and polytetrafluoroethylliner liner is put into stainless steel outer sleeve and placed the constant temperature air dry oven with temperature programming function, is warmed up to 180 ℃ of reactions 12 hours;
(3) aftertreatment: after reaction finishes, close the constant temperature air dry oven and naturally cool to room temperature, use deionized water and absolute ethyl alcohol wash products successively after, sample placed under the room temperature dries naturally; The sulphur indium zinc film sample that obtains is carefully changed in the sample bottle, in lucifuge, exsiccant environment, preserve.Product colour is that glassy yellow shows slightly metalluster, and the microtexture under electron microscope is latticed nanocrystalline, but has part metals not have complete reaction.Electron photomicrograph is seen Fig. 3.
Embodiment 3
(1) preparation work: with embodiment 2;
(2) reactions step: put into polytetrafluoroethylliner liner to the ITO conductive glass substrate of handling with nanometer indium zinc alloy surface; Add the sulphur powder; The height that adds anhydrous ethanol solvent to container 75% then; Sulphur powder concentration is 0.0015 grams per milliliter, and polytetrafluoroethylliner liner is put into stainless steel outer sleeve and placed the constant temperature air dry oven with temperature programming function, is warmed up to 160 ℃ of reactions 24 hours;
(3) aftertreatment: after reaction finishes, close the constant temperature air dry oven and naturally cool to room temperature, use deionized water and absolute ethyl alcohol wash products successively after, sample placed under the room temperature dries naturally; The sulphur indium zinc film sample that obtains is carefully changed in the sample bottle, in lucifuge, exsiccant environment, preserve.Product colour is that glassy yellow shows slightly metalluster, and the microtexture under electron microscope is latticed nanocrystalline but have part metals not have complete reaction.Electron photomicrograph is seen Fig. 4.
Embodiment 4
(1) preparation work: with embodiment 3;
(2) reactions step: put into polytetrafluoroethylliner liner to the ITO conductive glass substrate of handling with nanometer indium zinc alloy surface; Add the sulphur powder; The height that adds anhydrous ethanol solvent to container 75% then; Sulphur powder concentration is 0.0015 grams per milliliter, and polytetrafluoroethylliner liner is put into stainless steel outer sleeve and placed the constant temperature air dry oven with temperature programming function, is warmed up to 180 ℃ of reactions 24 hours;
(3) aftertreatment: after reaction finishes, close the constant temperature air dry oven and naturally cool to room temperature, use deionized water and absolute ethyl alcohol wash products successively after, sample placed under the room temperature dries naturally; The sulphur indium zinc film sample that obtains is carefully changed in the sample bottle, in lucifuge, exsiccant environment, preserve.Product colour is a glassy yellow, and the microtexture under electron microscope is latticed nanocrystalline.Electron photomicrograph is seen Fig. 5.
Embodiment 5
(1) preparation work: with embodiment 4;
(2) reactions step: put into polytetrafluoroethylliner liner to the ITO conductive glass substrate of handling with nanometer indium zinc alloy surface; Add the sulphur powder; The height that adds anhydrous ethanol solvent to container 75% then; Sulphur powder concentration is 0.001 grams per milliliter, and polytetrafluoroethylliner liner is put into stainless steel outer sleeve and placed the constant temperature air dry oven with temperature programming function, is warmed up to 180 ℃ of reactions 24 hours;
(3) aftertreatment: after reaction finishes, close the constant temperature air dry oven and naturally cool to room temperature, use deionized water and absolute ethyl alcohol wash products successively after, sample placed under the room temperature dries naturally; The sulphur indium zinc film sample that obtains is carefully changed in the sample bottle, in lucifuge, exsiccant environment, preserve.Product colour is a glassy yellow, and the microtexture under electron microscope is latticed nanocrystalline.Electron photomicrograph is seen Fig. 6.
The present invention directly adopts elemental sulfur and the ITO conductive glass substrate that is coated with the indium zinc alloy to prepare the nano mesh-like sulfur-indium-zinc ternary compound optoelectronic thin-film material through single step reaction, and uses the simplest anhydrous ethanol solvent as reaction medium.Belong to environmentally friendly reaction.The low-temperature original position growth good reproducibility, film is transparent, mesh nanometer structure and morphology homogeneous, perfection, the surface is very evenly smooth, has solved the uneven problem of other spin coating method crystal films.Of no use to any additive and tensio-active agent, do not need follow-up thermal treatment and purification step.Reaction is quick, and is easy to operate, is convenient to suitability for industrialized production and technology popularization.Because of its preparation facilities is simple, need not to carry out advantages such as aftertreatment and greatly reduce cost, will have wide practical use in area of solar cell.
Claims (2)
1. sulfur-indium-zinc ternary compound optoelectronic film material is characterized in that: this material is the netted ZnIn that is made up of nano flake of in-situ preparing in the ITO conductive glass substrate with nanometer indium zinc alloy surface
2S
4The ternary compound optoelectronic film material; Wherein nano flake thickness is 20～30nm, and this preparation methods is to place the tetrafluoroethylene reaction kettle to ITO conductive glass base material, elemental sulfur powder and anhydrous ethanol solvent with nanometer indium zinc alloy surface altogether, and the concentration of elemental sulfur powder is 0.001-0.0015 gram sulphur/milliliter anhydrous ethanol solvent; Reaction is 24 hours under 180 ℃ of temperature; Reaction naturally cools to room temperature after finishing, and final product cleans with deionized water and absolute ethyl alcohol successively; Naturally dry under the room temperature, promptly get.
2. sulfur-indium-zinc ternary compound optoelectronic film material as claimed in claim 1; It is characterized in that described ITO conductive glass base material with nanometer indium zinc alloy surface is meant the material that has plated one deck nanometer indium zinc alloy through ion sputtering at the ITO conductive glass surface.
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| CN102181847A (en) * | 2011-04-14 | 2011-09-14 | 山东大学 | Method for depositing Cu-Zn-Tin-Sulfur film by ethanol heat |
| CN102225847B (en) * | 2011-05-09 | 2012-11-21 | 浙江大学宁波理工学院 | Preparation method for porous In2S3 film |
| CN102887539B (en) * | 2012-09-24 | 2014-10-29 | 许昌学院 | Chemical method for performing in-situ preparation of nano sulfur-tin-zinc-copper quaternary compound photovoltaic film |
| CN103247718B (en) * | 2013-04-09 | 2015-06-17 | 许昌学院 | Chemical method for in-situ control and synthesis of AgCuS/Ag3CuS2 ternary semiconductor photoelectric thin-film material at normal temperature |
| CN107282070B (en) * | 2017-05-26 | 2020-01-10 | 上海纳米技术及应用国家工程研究中心有限公司 | Three-dimensional flower-shaped sulfur indium zinc micro-nanowire array and preparation method and application thereof |
| CN108409157A (en) * | 2018-03-19 | 2018-08-17 | 中国矿业大学 | A kind of ZnIn2S4 nanometer wafer arrays structure and preparation method thereof |
| CN108620105B (en) * | 2018-05-04 | 2021-02-12 | 福州大学 | Composite photocatalyst MxP/sulfur indium zinc and preparation method and application thereof |
| CN109052988B (en) * | 2018-10-19 | 2022-04-05 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of zinc indium sulfide nanosheet array film |
| CN109621979B (en) * | 2018-12-13 | 2021-09-21 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of ZnO/zinc indium sulfide nano heterojunction |
| CN111822013B (en) * | 2020-07-06 | 2022-11-18 | 重庆大学 | Single-cell PN junction and accurate construction method thereof |
| CN114894874B (en) * | 2022-04-18 | 2023-02-14 | 湖南大学 | Self-powered double-optical-electrode sensor and preparation method and application thereof |
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| CN100545081C (en) * | 2007-07-12 | 2009-09-30 | 许昌学院 | Dendritic silver selenide nano crystal thin film material and preparation method |
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| CN100545081C (en) * | 2007-07-12 | 2009-09-30 | 许昌学院 | Dendritic silver selenide nano crystal thin film material and preparation method |
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| 李明涛等.ZnIn2S4薄膜喷雾热分解制备及其光电化学性质.《西安交通大学学报》.2008,第42卷(第1期),第106-109页. * |
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